High temperature high pressure apparatus



June 21, 1960 F. P. BUNDY 2,941,243

HIGH TEMPERATURE HIGH PRESSURE APPARATUS Filed Feb. 14. 1955 In v enter": Francis 7? Bundy,

by 204! d M His A t y HIGH TEMPERATURE HIGH PRESSURE APPARATUS Francis P. Bondy, Alplaus, N.Y., assignor to General Electric Company, a corporation of New York Filed Feb. 14, 1955, Ser. No. 488,042

7 Claims. (Cl. 1816.5)

high temperatures and high pressures are maintained for prolonged periods of time.

An apparatus which is capable of producing temperatures of the order of several thousand degrees centigrade. and pressures of the order of 20,000 to 40,000 atmospheres for long time intervals is desirable to effect and control reactions occurring under such conditions. Vessels with such a high internal pressure range must be carefully designed to avoid explosive rupture even at room temperature. Such design and construction problems are greatly increased when high pressure apparatus is subjected to high temperatures of the order mentioned. The invention of the present application provides an ap paratus which produces concurrent high temperatures and high pressures of such orders for sustained time intervals without rupturing of the device.

Accordingly, it is an object of my invention to provide a new and improved high temperature high pressure ap paratus.

It is another object of the invention to provide a compact apparatus for heating and pressing a specimen.

It is a further object of the invention to provide an improved high temperature high pressure apparatus which is economically manufactured and assembled.

In carrying out my invention in one form, a reaction vessel is positioned between a pair of opposed, recessed dies to provide a specimen chamber which is subjected to high temperature and high pressure.

These and various other objects, features and advantages of the invention will be better understood from the following description taken in connection with the accompanying drawing in which:

Fig. 1 is a front elevational view of a hydraulic press with a high temperature high pressure apparatus which embodies my invention;

Fig. 2 is an enlarged sectional view of the high temperature high pressure apparatus which is shown in Fig. 1; and

Fig. 3 is a modified high temperature high pressure apparatus.

In Fig. l of the drawing, a hydraulic press comprises a base 10 with a press bed 11 on which is mounted a plurality of vertical shafts 12 to support a carriage 13 with a shaft 14. A pair ofopposed pistons 15 and 16 on bed 11 and carriage 13 are recessed to partially position members 17 therein each of which comprises a central die 18 with surrounding binding rings 19. A layer of electrical insulation 20 is provided between at least one member 17 and its associated piston 15 to prevent conduction of electric current through the press. An electrical connection to each member 17 is provided by a conducting ring 21 with a connector 22 which ring is positioned around the periphery of each outer binding ring 19 to supply electric current from a source of power not shown) through rings 19 and dies 18 to the high 2,941,243 Patented June 21, 1960 temperature high pressure reaction vessel which is described below. I

As is best shown in Fig. 2, the outer face of each die 18 has a raised annular lip 23 which surrounds and defines a recess in the center of the outer face of each die. A block 24 of electrically insulating material is positioned in the central portion of each recess to prevent burning out dies 18 through the application of current thereto. A reaction vessel 25, which is located within the recesses of opposing dies 18, comprises a pair of spaced conductive discs 26 with a hollow conductive cylinder 27 therebetween adapted to contain a specimen 28 to be subjected to high temperature high pressure conditions. An annular washer 29 of electrically insulating material is positioned around cylinder 27 between discs 26 to complete the assembly of reaction vessel 25. If it is desired, vessel 25 may be in the form of a hollow casing which is in electrical contact with opposing dies 18. I have also found that maximum pressures are secured when the reaction vessel has a diameter of the order of several times its axial thickness. An annular thermal and electrically insulating and pressure resisting washer 30 surrounds the side of vessel 25 to confine heat and pressure within cylinder 27. Washer 30 is tapered laterally and arranged to have its outer edge fit between and be engaged by lips 23 of dies 18 to prevent lateral extrusion thereof with attendant loss of pressure to vessel 25. Examples of suitable materials from. which blocks 24 and washers 29 and 30 may be made are pyrophyllite and catlinite.

In the operation of the high temperature high pressure apparatus shown in Figs. 1 and 2, each member 17 with associated conducting ring 21 and connector 22 is positioned partially within the recess of its respective piston in the press. Block 24 is then set in the recess of each die 18 to provide electrical insulation. Specimen 28 which is to be subjected to a high temperature high pressure environment is placed in cylinder 27 within washer 29 and between discs 26 to complete reaction vessel 25. Washer 30 is placed around vessel 25 after which this vessel and its associated washer are positioned within the recesses of opposing dies 18 between blocks 24. The outer edge of washer 30 fits between and is engaged by opposed lips 23 to prevent lateral extrusion of this washer with attendant loss of pressure to vessel 25 when pressure is applied by the press.

Pressure is applied to specimen 28 in cylinder 27 by shaft 14 of the press. At the same time, electric current is supplied from one electrical connector, such as upper connector 22, to upper conduct-ing ring 21, binding rings 19, die 18 and disc 26 to generate heat in cylinder 27 of vessel 25. The current path continues from cylinder 27 through lower disc 26, die 18, binding rings 19, conducting ring 21, and connector 22 to the electrical source. Pressures in excess of 35,000 atmospheres at I temperatures higher than 2500 C. have been maintained in such apparatus for periods of hours. If it is desired, reaction vessel 25 may also be subjected to high pressure alone. 1

In Fig. 3 of the drawing, a modified high temperature high pressure apparatus is shown in which the reaction vessel with'washer 30 is surrounded by a compressible electrically insulating gasket 31 with yielding characteristics, such as rubber or plastic. Gasket 31 is positioned between lips 23 and the outer edges of opposing dies- 18 to engage the gasket inner edge between such opposin'g lips; Soft steel retaining rings 32 are positioned around the periphery of gasket 31 to slide with respectto each other during closure of dies 18. A layer 33 of insulatingmaterial is also provided between at least one ring 32 and its associated die 18 to prevent short-circuiting the flow of current through cylinder 27 of the press 'Iheoperation of apparatus in vFig. 3 is similar to apparatus in Fig. 2 with the exception that closure of dies 18 exerts pressure against gasket 31 with a circumferential stretching of rings 32 to provide a back pressure which regulates compressive loading of dies 18. Stress concentration is relieved near the surfaces of dies 18. with a resulting increase in maximum compressive loading in cy in r .27.-

As will be apparent to. those skilled in the art, the objects of my invention are attained by the use of a reaction vessel which is positioned between a pair of opposed, recessed dies to provide a specimen chamber to be subjected to high temperature and high pressure conditions.

While other modifications of this invention and variations of apparatus have not been described, the invention is; intended to include all such as may be embraced within the following claims.

What I claim as new and desire to secure by Letters Patent of the United States is:

1. High temperature high pressure apparatus. comprising a. pair of opposed, recessed pistons, means for exerting pressure against at least one of said pistons, a pair of members, each of said members being positioned partially within each of said recesses, a layer of insulation between one of said members and its associated piston, an electrical connection to each of said members, each member comprising a die, the outer face of said die having a raised annular lip defining a recess, a substantially cylindrical reaction vessel located within the recesses of opposing die faces, the ends of said reaction vessel being in electrical contact with said dies, and an annular insulating and pressure resisting washer surrounding the side of said vessel, said washer having its outer edge positioned adjacent said annular lip, the outer edge of said washer being arranged to fit between and be engaged by the lips of said dies.

2. High temperature high pressure apparatus comprising a pair of opposed, recessed pistons, means for exerting pressure against at least one of said pistons, a pair of members, one of said members being positioned partially within each of said recesses, a layer of insulation between one of said members and its associated piston, an electrical connection to each of said members, each member comprising a die, the outer face of said die having a raised annular lip defining a recess, a reaction vessel located within the recesses of opposing die faces, said reaction vessel comprising a hollow conductive cylinder adapted to contain a specimen to be subjected to high temperature high pressure conditions in electrical contact with said dies, said vessel having a diameter of the order of several times its axial thickness, and an annular insulating and pressure resisting washer surrounding the side of said vessel, said washer having its outer edge positioned adjacent said annular lip, the outer edge of said washer being arranged to fit between and be engaged by the lips of said dies.

3. High temperature high pressure apparatus comprising a pair of opposed, recessed pistons, means for exerting pressure against at least one of said pistons, a pair of members, one of said members being positioned partially within each of said recesses, a layer of insulation between one of said members and its associated piston, an'electrical-eonnection to each of said members, each member comprising a die, at least one binding ring. around said die, the outer face of said die having a raised annular lip defining a recess, a block of electrically insulating material positioned in the central portion of said recess, a reaction vessel located within the recesses of opposing die faces between said blocks, said reaction vessel comprising a hollow conductive cylinder adapted to contain a specimen to be subjected to high temperature high pressure conditions in electrical contact with said dies, said vessel having a diameter of the order of several times its :axial thickness, and an annular insulating and pressure resistingwasher surrounding the side of said vessel, said i washer having its outer edge positioned adjacent said annular lip, the outer edge of said washer being arranged to fit between and be engaged by the lips of said dies.

4. High temperature high pressure apparatus comprising a pair of opposed, recessed pistons, means for exerting pressure against at least one of said pistons, a pair of members, each of said members being positioned partially within-each of said recesses, a layer of insulation between one of said members and its associated piston, an electrical connection to each of said members, each member comprisinga die, at. least one binding ring around said die, the outer face of said die having a raised annular lip defining a recess, a block of electrically insulating material positioned in the central portion of said recess, a reaction vessel located within the recesses of opposing die faces between said blocks, said reaction vessel comprising a pair of spaced conductive discs, a hollow conductive cylinder adapted to contain a specimen to be subjected to. high temperature high pressure conditions positioned between said discs, an annular insulating washer around said cylinder between said discs, said vessel having a diameter of the order of several times its axial thickness, and an annular insulating and pressure resisting Washer surrounding the side of said vessel, said insulating and pressure resisting. washer having its outer edge positioned adjacent said annular lip, the outer edge of said insulating and pressure resisting washer being arranged to fit between and be engaged by the lips of said dies.

5. High temperature high pressure apparatus comprising a pair of'opposed, recessed pistons, means for exerting pressure against atleast one of said pistons, a pair of members, each of said members being positioned partially within each of said recesses, a layer of insulation between one of said members and its associated piston, an electrical connection to each of said members, each member comprising a die, at least one binding ring around said die, the outer face of said die having a raised annular lip defining a recess, a block of electrically insulating material positioned in the central portion of said recess, a reaction vessel located within the recesses of opposing die faces between said blocks, said reaction vessel comprising a pair of spaced conductive discs, a hollow conductive cylinder adapted to contain a specimen to be subjected to high temperature high pressure conditions positioned between said discs, an annular insulating washer around said cylinder'between said discs, said vessel having a diameter of the order of several times its axial thickness, an annular insulating and pressure resisting washer surrounding the side of said vessel, said insulating and pressure resisting Washer having its outer edge positioned adjacent said annular lip, the outer edge of said insulating and pressure resisting was-her being arranged to fit between and be engaged by the lips of said dies, an annular compressible insulating gasket arranged to surround said washer between the lips and outer edges of opposing die faces, said gasket having an inner edge positioned to be engaged by said opposing lips, and a pair of slidably opposed retaining rings around the periphery of said gasket between said dies, at least one of said rings being insulated from its adjacent die.

6. A high pressure, high temperature apparatus comprising in combination, a pair of opposed dies, a raised annular tapered lip on the opposing surface of each die, the said lips on each die being adapted to meet in opposed relationship, and defining a recess to contain an object to be subjected to high pressures and high temperatures, an annular thermal and electrical insulating gasket surrounding and engaging said object and being engaged by said lips, and means to move one of said dies toward the other.

7. A high pressure, high temperature apparatus comprising in combination, a pair of opposed dies, a raised annular tapered lip on the opposing surface of each die, the said lips being in opposed relationship and defining a recess, a bloek of thermal and electrically insulating material in said recess in each die, a reaction vessel posi- OTHER REFERENCES tioned in said recess between said blocks, said reaction u vessel comprising a thermal and electrically insulating ga ggggg i g Physlcs' 2 (Feb' hollow cylinder adapted to contain a specimen to be sub- Q t jected to high pressures and high temperatures, an elec- 5 i i f g f fifg gf g 3222 2 jgi fig g f trically conductive metal disc covermg each end of said 1952 cylinder and in electrical contact with said die, an annut I lar thermal and electrical insulating gasket surrounding 53:3 6 5 3 23551 gg ggg $5 2% and engaging said reaction vessel and being engaged by 92401 said lips, and means for conducting electrical current to 10 Bridgmam Acad of Arts and Sciences Proceed said ings, vol. 74, N0. 3, pages 21-28, Oct. 1940.

References Cited in the tile of this patent p g ggg fi g' zgi Anorg- Chem" UNITED STATES PATENTS Bridgman: Review of Modern Physics, vol. 18, No.

2,544,414 Bridgman et a1 Mar. 6, 1951 15 1, pages 1-9, 25, 34, 79=88 (1946). 

